Investigating the crystallinity of hard candies prepared and stored at different temperatures with low field-NMR relaxometry.

BACKGROUND: In this study, hard candies were produced by using sucrose, glucose syrup and water. They were cooked at different temperatures, changing from 135 to 145 °C with an interval of 2.5 °C. They were stored at different storage temperatures, which were 25, 4, -18 and -80 °C. Hard candies placed at room temperature were stored for 2 months. In order to understand the crystallization characteristics of the hard candies, time domain (TD) proton nuclear magnetic resonance (1H-NMR) parameters of longitudinal relaxation time (T1) and second moment (M2) measurements were conducted. Moisture contents of the hard candies were determined by Karl-Fischer titration. X-ray diffraction experiments were also conducted as the complementary analysis. RESULTS: Increasing cooking temperature increased the crystallinity and decreased the moisture content of the hard candies significantly (P ≤0.05). Furthermore, storage temperature and storage time had significant effects on the crystallinity of the hard candies (P ≤0.05). The results of T1 and M2 correlated with each other (r > 0.8, P ≤ 0.5) and both produced the highest value at the cooking temperature of 145 °C and storage temperature of 4 °C (P ≤ 0.05). The values of T1 and M2 were obtained as 245.9 ms and 13.0 × 10-8 Hz2, respectively, for the cooking temperature of 145 °C and storage temperature of 4 °C. CONCLUSION: This study demonstrated that the crystallinity of hard candies can be observed and examined by TD-NMR relaxometry, as an alternative to commonly used methods. © 2024 The Author(s). Journal of the Science of Food and Agriculture published by John Wiley & Sons Ltd on behalf of Society of Chemical Industry.

Effect of microwave-vacuum drying on the physicochemical properties of a functional tomato snack bar.

BACKGROUND: Tomato is an indispensable ingredient of the Mediterranean diet. Reformulation of traditional Mediterranean products to increase the adherence of consumers is becoming popular. In this study, a tomato snack bar enriched with olive powder and pea protein was developed by using microwave-vacuum drying. Formulations also included tomato powder (TP) and low-methoxylated pectin (LMP) as a structuring agent. RESULTS: The moisture content of microwave-vacuum-dried samples varied in the range 13.6-19.8% and water activity (aw ) values were ~0.6. LMP and TP concentrations affected the color of microwave-vacuum-dried samples. However, the color mainly changed in conventionally dried samples due to browning. In microwave-vacuum-dried samples, lycopene content decreased with increasing LMP, but increased with increasing TP. Textural properties of microwave-vacuum-dried snack bars increased with increasing LMP and TP. CONCLUSION: Both texture and Fourier transform infrared spectroscopy results indicated that there was a network formation due to the contribution of protein and pectin; however, the type of interaction was highly dependent on the drying mechanism. Nuclear magnetic resonance relaxometry data showed that microwave-vacuum-dried samples had a more uniform water distribution. Besides its time and energy efficiency, microwave-vacuum drying improved the color and textural properties of tomato snack bars compared to conventionally dried ones. © 2023 The Authors. Journal of The Science of Food and Agriculture published by John Wiley & Sons Ltd on behalf of Society of Chemical Industry.

Non-Conventional Time Domain (TD)-NMR Approaches for Food Quality: Case of Gelatin-Based Candies as a Model Food.

The TD-NMR technique mostly involves the use of T1 (spin-lattice) and T2 (spin-spin) relaxation times to explain the changes occurring in food systems. However, these relaxation times are affected by many factors and might not always be the best indicators to work with in food-related TD-NMR studies. In this study, the non-conventional TD-NMR approaches of Solid Echo (SE)/Magic Sandwich Echo (MSE) and Spin Diffusion in food systems were used for the first time. Soft confectionary gelatin gels were formulated and conventional (T1) and non-conventional (SE, MSE and Spin Diffusion) TD-NMR experiments were performed. Corn syrups with different glucose/fructose compositions were used to prepare the soft candies. Hardness, °Brix (°Bx), and water activity (aw) measurements were also conducted complementary to NMR experiments. Relaxation times changed (p < 0.05) with respect to syrup type with no obvious trend. SE/MSE experiments were performed to calculate the crystallinity of the samples. Samples prepared with fructose had the lowest crystallinity values (p < 0.05). Spin Diffusion experiments were performed by using Goldman−Shen pulse sequence and the interface thickness (d) was calculated. Interface thickness values showed a wide range of variation (p < 0.05). Results showed that non-conventional NMR approaches had high potential to be utilized in food systems for quality control purposes.

Water Dynamics in Whey-Protein-Based Composite Hydrogels by Means of NMR Relaxometry.

Whey-protein-isolate-based composite hydrogels with encapsulated black carrot (Daucus carota) extract were prepared by heat-induced gelation. The hydrogels were blended with gum tragacanth, pectin and xanthan gum polysaccharides for modulating their properties. 1H spin-lattice relaxation experiments were performed in a broad frequency range, from 4 kHz to 30 MHz, to obtain insight into the influence of the different polysaccharides and of the presence of black carrot on dynamical properties of water molecules in the hydrogel network. The 1H spin-lattice relaxation data were decomposed into relaxation contributions associated with confined and free water fractions. The population of the confined water fraction and the value of the translation diffusion coefficient of water molecules in the vicinity of the macromolecular network were quantitatively determined on the basis of the relaxation data. Moreover, it was demonstrated that the translation diffusion is highly anisotropic (two-dimensional, 2D).

Physicochemical and sensorial properties of tomato leathers at different drying conditions.

Tomato leather as a healthy alternative to traditional fruit leathers was formulated. A tray dryer with changing temperature (50, 60, and 70°C) and relative humidity (5%, 10%, and 20%) was used to achieve the best product in terms of color, water distribution, lycopene content, mechanical, and sensorial properties. Color change was the highest at 70°C due to the Maillard reaction. Lycopene content was also the highest at 70°C. Time domain-NMR relaxometry showed that water distribution of all samples was homogeneous and similar to each other. Processing conditions affected mechanical properties significantly. The highest tensile strength was observed at 70°C, possibly due to the denatured proteins. Sensory analysis indicated better flavor development at 70°C, whereas overall acceptability of samples was higher at 50°C. The results of this study showed the main processing parameters of tomato leather with a minimal amount of ingredients, with acceptable mechanical and sensorial properties. PRACTICAL APPLICATION: Tomato leather was produced by using minimal amount of ingredients. Taste of the leather was found acceptable, as a salty snack food. Therefore, this product can be produced economically and it has a high potential to be consumed as an alternative to conventional fruit leathers.

Hard Candy Production and Quality Parameters: A review.

Hard candies are sugar confections comprising mainly water and sucrose. Corn syrup, colorants and flavors are also usually added to hard candy formulations. The production of hard candy requires heating of the ingredients to very high temperatures to reduce moisture content and subsequent cooling to obtain a solid matrix. Cooling of the mixtures achieves the final, well known glassy state of the products. In this glassy state, the system is kinetically stable and molecular mobility is restricted, providing longer shelf life to hard candies. There are, however, several factors affecting the final quality and consumer acceptance of hard candies. Production methods and parameters, initial formulations as well as storage conditions all play a crucial role in the physicochemical, textural and sensory properties of hard candies. Addition of colorants and flavors also plays a vital role in the final quality. Although hard candy production is a simple process with few production stages, even small changes in the method of production and process parameters may induce substantial changes in the final product characteristics. Additionally, storage conditions such as temperature and humidity can change the product properties leading to graining and stickiness which are the two major problems for hard candies during storage. Both production and storage conditions should therefore be carefully chosen and controlled for desirable hard candy properties. This review addresses the general production methods and considers process parameters and quality parameters of hard candy products. Moreover, a comprehensive review of the related hard candy literature is also presented. The majority of hard candy reviews focus on specific methods and processes, but this review will present a more general frame on the subject.

Challenges in dried whey powder production: Quality problems.

Whey is a high nutritional value by-product of the dairy industry. It is generally produced in large quantities and its disposal as wastewater poses environmental risks. For this reason, whey streams are used for the production of value-added products such as dried whey powders. However, there are several challenges related to whey processing that lead to low powder yield and quality, especially caking. These challenges can be addressed by optimization of product formulation and processing parameters. In this review, we discuss the effects of dried whey protein powder production stages and process parameters on the quality of the final powder product. The initial composition of whey used for dried whey powder production affects the final quality of the product. Generally, a high mineral and/or lactic acid content is not desirable since these constituents cause lactose-containing whey particles to adhere to the drying equipment surfaces, thereby reducing the powder yield. An effective lactose pre-crystallization is essential since high amorphous lactose content increases the stickiness of the dried-whey powder particles and induces caking during storage. Therefore, whey should undergo filtration and lactose pre-crystallization before spray drying. Studies show that it is possible to retard caking and improve the quality attributes of dried whey powders by optimizing the product formulation and processing operations.

Physical characterization of high methoxyl pectin and sunflower oil wax emulsions: A low-field 1 H NMR relaxometry study.

Pectin-wax-based emulsion systems could be used to form edible films and coatings with desired water permeability characteristics. Pectin is often used in food industry due to its gelling and viscosity increasing properties. Physical properties of pectin are highly dependent on its esterification degree. Waxes are commonly used as edible coatings to enhance the water barrier properties of food products. This study focuses on preparing emulsions with sunflower oil wax (SFW) and high methoxyl pectin (HMP) at different concentrations for any possible edible film or coating formulations. Sunflower oil (SFO) was added as the dispersed oil phase to these emulsions. Characterization of the emulsions was performed by using particle size, rheology, and time domain nuclear magnetic resonance (NMR) relaxometry measurements. Effects of HMP concentration and the presence of SFO in the emulsion formulations were explored. Mean particle size values were recorded between 1 and 3 µm. Rheology measurements showed that increasing HMP concentrations and presence of SFO in emulsions resulted in more pseudoplastic behavior. NMR transverse relaxation times (T2 ) were measured to detect the differences between the emulsions. Relaxation spectrum analysis was also conducted for a detailed understanding of the transverse relaxations. Addition of SFO and higher HMP concentrations decreased the T 2 values of the emulsion systems (P < 0.05). However, T2 decreasing effect of SFO was compensated at 10% (w/w) HMP concentration showing that SFO was well dispersed in this particular emulsion formulation. Changes in the rheological behavior and relaxation times provided insight on the formation and stability of the emulsions. PRACTICAL APPLICATION: Findings of this study can be utilized and integrated to produce edible films and coatings with different water permeability characteristics. This study showed that NMR relaxometry parameters were also effective in monitoring and determining the physical characteristics of the pectin-wax-based emulsion systems as other conventional techniques including rheology and particle size measurements. Our NMR relaxometry findings were in correlation with the flow behavior and particle size results of the investigated emulsion systems.

The effects of pectin and wax on the characteristics of oil-in-water (O/W) emulsions.

The study was aimed to investigate characteristics of emulsion containing pectin, wax, maltodextrin, and carotenoid enriched flaxseed oil by means of stability, rheology, particle size, and low-resolution of time domain nuclear magnetic resonance (NMR) relaxometry measurements. Emulsions were prepared with different carotenoid enriched-flaxseed oil concentrations (6%, 9%, 12%, and 15% w/w) and ratios of maltodextrin/(pectin+wax) (3:1, 6:1, 9:1, and 12:1 g/g). Percentage separation of 12% oil 12:1 ratio of maltodextrin/(pectin+wax) (g/g), 15% oil 9:1, and 12:1 ratios of maltodextrin/(pectin+wax) (g/g) of emulsions was determined as 2.0 ± 0.5%, 4.0 ± 0.5%, and 8.0 ± 0.5%, respectively. No separation was observed in other emulsions. The rheological behavior of emulsions was best described by the power law model. When the concentration of pectin+wax in the emulsion decreased, the n values of the emulsions were close to 1, indicating that the fluid behavior approaches Newtonian behavior. Moreover, the emulsion viscosity was observed to increase when pectin and wax concentrations in the emulsion increased. The increase in pectin and wax concentration in emulsions with oil contents of 6% and 9% resulted in a reduction in the average particle size. However, if the oil concentration in the emulsions was 12% or more, the increase in the ratio of maltodextrin/(pectin+wax) (g/g) led to a decrease in the average particle size. NMR transverse relaxation times (T2 ) of emulsions were measured and results showed that T2 values for almost all formulations decreased when the ratio of maltodextrin/(pectin+wax) reduced. PRACTICAL APPLICATION: Study results demonstrated that the combination of pectin and wax together with maltodextrin as a filling material could be an alternative way to improve emulsion stability. Findings of this study provided useful guidance for the future studies about the potential use of pectin, wax, and maltodextrin as wall material in encapsulation of oils or in producing edible films.

In vitro digestion of polysaccharide including whey protein isolate hydrogels.

Hydrogels are great systems for bioactive agent encapsulation and delivery. In this study, polysaccharide blended whey protein isolate (WPI) based hydrogels were loaded with black carrot (Daucus carota) concentrate (BC) and in vitro gastrointestinal release measurements were performed. Prior to 6 h digestion in simulated intestinal fluid (SIF), all hydrogels were exposed to simulated gastric fluid (SGF) for 2 h. Pectin (PC), gum tragacanth (GT) and xanthan gum (XG) were the polysaccharides used with WPI to manipulate the release behavior. Physico-chemical changes of the hydrogels throughout the digestion were evaluated by Fourier transform infrared (FTIR) spectroscopy and nuclear magnetic resonance (NMR) relaxometry measurements. Each polysaccharide induced different physico-chemical interactions within the hydrogels due to their distinct structural characteristics. Polysaccharide blending to hydrogels also retarded the release rates in all samples in SIF (p < 0.05). Moreover, microstructural differences between hydrogels were evaluated by scanning electron microscope (SEM) images.

NMR Relaxometry and magnetic resonance imaging as tools to determine the emulsifying characteristics of quince seed powder in emulsions and hydrogels.

Quince seed powder (QSP) is known to exhibit emulsification properties and could be used as a natural emulsifier in colloidal food systems. In this study, emulsion-based alginate hydrogels were formulated using QSP and xanthan gum (XG) as stabilizers. The objective of the study was to show the emulsifying power of QSP in emulsions and their hydrogels using Time Domain (TD) NMR Relaxometry and Magnetic Resonance Imaging (MRI). Rheology and mean particle size measurements for emulsions and scanning electron microscope (SEM) experiments for hydrogels were further conducted as complementary methods. QSP containing emulsions were found to have longer T2 relaxation times than XG samples (p < 0.05). Addition of either QSP or XG produced a more pseudoplastic flow behavior (p < 0.05) on the emulsions. Relaxation times were also obtained by MR images through T2 maps. Relaxation decay curves showed the presence of two proton compartments in hydrogels; protons associated with the polymer matrix and protons interacting with the oil phase. The contribution of the first proton pools was the largest in QSP hydrogels confirmed by the lowest standard deviation in the T2 maps. This behavior was explained by the emulsification ability of QSP. Results showed that NMR Relaxometry and MR images could be used to understand the emulsifying nature of QSP and many other hydrocolloids.

Digestion of animal- and plant-based proteins encapsulated in κ-carrageenan/protein beads under simulated gastrointestinal conditions.

In this study, we encapsulated both animal-derived (whey) and plant-derived (soy and pea) proteins within polysaccharide/protein beads and measured the digestion of these beads under simulated gastrointestinal tract (GIT) conditions. Bead dimensions were measured using a digital caliper and found to increase as the shear thinning behavior of the protein/polysaccharide solutions used to form them increased. The hydrolysis of the plant and animal proteins trapped inside the protein/polysaccharide beads was studied using the pH-stat automatic titration method under simulated static GIT conditions. The encapsulated proteins were relatively resistant to digestion under gastric conditions, with only about 10 to 13% of the protein being digested by the end of the stomach phase. Conversely, they were almost fully digested under small intestinal conditions, with around 87 to 97% of the protein being hydrolyzed by the end. Indeed, by the completion of the small intestine phase, only "ghost" beads remained that contained cross-linked polysaccharides. The soy and pea proteins were digested slightly faster than the whey proteins in the stomach phase (p < 0.05), whereas the pea proteins were digested slightly faster than the soy and whey proteins under intestinal conditions (p < 0.05). Raman spectroscopy and scanning electron microscopy showed that there were changes in the composition and structure of the beads throughout the simulated GIT. Our results indicate that the gastrointestinal behavior of proteins can be modulated by encapsulating them in polysaccharide beads, which may be useful for the design of certain types of functional foods. Even so, the beads formed from the plant-based and animal-based proteins behaved fairly similarly, suggesting that animal proteins could be replaced by plant-based ones for this purpose.

Physico-Chemical Changes of Composite Whey Protein Hydrogels in Simulated Gastric Fluid Conditions.

Polysaccharide blended whey protein isolate (WPI) hydrogels were developed for the delivery of black carrot ( Daucus carota) concentrate as bioactive agent in simulated gastric fluid (SGF). Pectin (PC), gum tragacanth (GT), and xanthan gum (XG) were blended as additional polymers to modulate the release characteristics of the WPI hydrogels. Experiments showed that sole whey protein (C), XG, and GT blended hydrogels possessed restricted release profiles 67%, 61%, and 67%, respectively, whereas PC samples attained higher release rates (83%) ( p < 0.05). Interactions between polymers and aqueous medium were analyzed by nuclear magnetic resonance relaxometry. C (82 ms) and GT (84 ms) hydrogels attained higher T2 values than PC (74 ms) and XG (73 ms) samples in SGF. Hardness of only XG hydrogels increased from 1.9 to 4.1 N after gastric treatment. Physicochemical changes within hydrogels during release were also investigated, and hydrogels were proved to be appropriate for desired delivery purposes.